CN108069823A - A kind of method for preparing sugar alcohol co-producing white carbon black - Google Patents
A kind of method for preparing sugar alcohol co-producing white carbon black Download PDFInfo
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- CN108069823A CN108069823A CN201711072210.1A CN201711072210A CN108069823A CN 108069823 A CN108069823 A CN 108069823A CN 201711072210 A CN201711072210 A CN 201711072210A CN 108069823 A CN108069823 A CN 108069823A
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- sugar alcohol
- white carbon
- carbon black
- producing white
- solution
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
- C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
- C07C29/141—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
It is as follows including step the present invention relates to a kind of method for preparing sugar alcohol co-producing white carbon black：Raw material sugar with water-soluble strong base solution is mixed, adds in silicon, catalyst, deoxygenation is enclosed within 100~200 DEG C and is stirred to react；Filtering, obtains liquor C and filter residue D；Liquor C adds in acid, adjusts pH, is stirred to react, and filters, obtains filtrate E and solid F, solid F is dried, obtains white carbon；By filtrate E through electrodialysis desalination, sugar alcohol solution G is obtained, sugar alcohol solution G is concentrated, spray drying obtains sugar alcohol.The present invention is reducing agent using the hydrogen that silicon is generated with highly basic reaction, without being additionally passed through hydrogen or the other reducing agents of addition；Unreacted substance and product can reuse, and be polluted without " three wastes ", and for the sugar alcohol purity of preparation up to more than 90%, white carbon reaches 3,061 2009 A class standards of HG/T.
Description
Technical field
The present invention relates to a kind of methods for preparing sugar alcohol co-producing white carbon black, belong to sugar alcohol and white carbon preparing technical field.
Background technology
Sugar alcohol be sugar through catalytic hydrogen reduction be corresponding polyalcohol.Although sugar alcohol is not sugar however, appearance and performance are equal
There are many similarities with sugar.The sugariness of sugar alcohol is less than sucrose, and heat also mostly less than sucrose, accordingly acts as low sugariness, low-heat
The sweetener of amount or the filler of high-intensity sweeteners.Meanwhile they will not cause blood glucose generally all from the restriction of insulin
The rise of value, therefore it is commonly used for diabetes, the sweetener of obesity patient.In the oral cavity, this kind of sweetener is from microbial action,
Acid is not produced, therefore without saprodontia.Sugar alcohol can be used as nutrient carrier, carry mineral nutrient fast transportation in plant phloem.
And sugar alcohol improves the resistance of plant.Sugar alcohol be participate in intracellular penetration adjust important substance, plant salt damage, arid,
Under the environment stresses such as waterflooding, sugar alcohol can make plant adapt to adverse growth by adjusting cell permeability；Sugar alcohol can be improved to work
The resistance of property oxygen is avoided burning ultraviolet light day, plant-active oxygen injury caused by due to arid, disease, anoxic etc..
White carbon, chemical composition are hydrated SiO 2, are a kind of white, nontoxic, amorphous fine powders, are had more
Permeability, polymolecularity, light, chemical stability is good, high temperature resistant, do not burn, the excellent properties such as electrical insulating property is good it is important inorganic
Silicon compound.In paper industry, it can improve Paper White Degree, intensity and opacity, add the paper of white carbon, resistance to
The performances such as mill, feel, printing and gloss are better than being not added with the paper of white carbon.In pesticide industry, white carbon can be used as anti-caking
Agent, dispersant improve and absorb and spread performance.Advanced white carbon can be used as toothpaste abrasive and drug figuration dispersant.Hard charcoal
The black filler for being also used as the chemical products such as paint, ink, cosmetics, coating, plastics.
Chinese patent literature CN102071267A (application numbers：201010589328.3) one kind is disclosed with rice husk coproduction wood
The method of sugar, white carbon and activated carbon is rice husk by washing boiling, dilute acid hydrolysis xylose；Low-temperature carbonization, then reacted with concentrated base
Silica is extracted, white carbon is prepared using coprecipitation；Solid adds in liquor zinci chloridi low temperature and impregnates after a certain period of time, then passes through
High-temperature activation, pickling are washed to neutrality, and drying and grinding obtains activated carbon.The invention is using a Tiao Xian branches coproduction xylose, hard charcoal
Black and active carbon with high specific surface area, xylose use hemicellulose in continuous hydrolysis rice husk to prepare xylose process, improve xylose production
Rate is the preparation process of a more succinct feasible xylose, and white carbon uses a kind of chemical coprecipitation of evolution, by
Addition surfactant, which maintains precipitation particle, in solution system higher dispersion degree, has prepared high-purity, spherical hard charcoal
Black particle.Activated carbon is activated using chemical activation method, and activation temperature is low, advantageously forms the smaller carbon crystallite of size, can make
Produce that hole is more flourishing, the better activated carbon of absorption property；But the invention is added using volatile alcohol reagent and high temperature
Thermal bake-out, high energy consumption, and do not utilize environmental protection, it is most important that the xylose purity of production cannot ensure, and xylose need through
Sugar alcohol can be just obtained after crossing reduction, it is impossible to directly obtain sugar alcohol product.
By retrieval, do not find that the correlation for the white carbon that can be produced high-purity sugar alcohol but also prepare large specific surface area is literary
It offers.
It is it is therefore proposed that of the invention.
The content of the invention
In view of the deficiencies of the prior art, it is of the invention the present invention provides a kind of method for preparing sugar alcohol co-producing white carbon black
Sugar alcohol purity is high, white carbon large specific surface area.Preparation method of the present invention has low raw-material cost, simple for process, environmentally friendly, Xun Huan
The advantages that utilization.
Technical solution of the present invention is as follows：
A kind of method for preparing sugar alcohol co-producing white carbon black is as follows including step：
Raw material sugar with water-soluble strong base solution is mixed, adds in silicon, catalyst, it is anti-that deoxygenation is enclosed within 100~200 DEG C of stirrings
It should；Filtering, obtains liquor C and filter residue D；
Liquor C adds in acid, adjusts pH, is stirred to react, and filters, obtains filtrate E and solid F, solid F is dried, obtains hard charcoal
It is black；
By filtrate E through electrodialysis desalination, sugar alcohol solution G is obtained, sugar alcohol solution G is concentrated, spray drying obtains sugar alcohol.
, according to the invention it is preferred to, the water solubility highly basic is sodium hydroxide or potassium hydroxide；
Preferably, in water-soluble strong base solution, the mass ratio of water-soluble highly basic and water is 0.1~0.5：1；Further preferably
, 0.2~0.4：1；
, according to the invention it is preferred to, the raw material sugar is glucose, xylose or fructose；
Preferably, the mass ratio of the raw material sugar and water in water-soluble strong base solution is 0.1~1：1；Further preferred 0.4
~1：1.
, according to the invention it is preferred to, the silicon is industrial silicon；
Preferably, the molar ratio of the silicon and water-soluble highly basic is 0.45~0.55：1；Further preferred 0.5~0.51：
1；
Preferably, the catalyst is Raney's nickel or palladium carbon, it is further preferred that Ni >=90wt% in Raney's nickel, palladium carbon
Middle Pd >=5wt%；
Preferably, the mass ratio of the catalyst and raw material sugar is 0.001~0.02：1；Further preferred 0.005~
0.015：1.
, according to the invention it is preferred to, silicon is added in, temperature is stirred to react as 110~170 DEG C under catalyst；Temperature
Spend low, silicon is substantially reactionless with potassium hydroxide, and temperature is excessively high, and reaction is violent, and pressure rise is rapid, and operation is unable to control；It stirs
Mix the reaction time for 2~for 24 hours；Further preferred 5~10h.
, according to the invention it is preferred to, the acid is sulfuric acid or hydrochloric acid；
Preferably, it is 6~7 to adjust pH；
Preferably, it is 40~90 DEG C to adjust the temperature being stirred to react after pH, and the reaction time is 30~90min.
According to the present invention, the method for preparing sugar alcohol co-producing white carbon black, a kind of preferred embodiment, including walking as follows
Suddenly：
(1) water-soluble highly basic and water are added in reaction kettle, stirring at normal temperature until no solid particle, obtains molten
Liquid A；
(2) raw material sugar is added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle,
Obtain solution B；
(3) silicon is added in the solution B of step (2) preparation, then adds in catalyst, deoxygenation is closed, in 100~200
It DEG C is stirred to react, after the completion of reaction, then liquor C and filter residue D is obtained by filtration, and filter residue D is recycled in cooling；
(4) acid is added in into liquor C, adjusts pH, heating is stirred to react, is filtered by filter, filtrate E is obtained by filtration
With solid F, solid F is dried, obtains white carbon；
(5) filtrate E is obtained into sugar alcohol solution G, solution G is concentrated, spray drying obtains sugar alcohol through electrodialysis desalination.
, according to the invention it is preferred to, oxygen removal process is with nitrogen displacement deoxygenation in step (3).
The hydrogen rationally generated in the above-mentioned preparation method of the present invention using silicon with highly basic reaction is reducing agent, and reduced sugar is sugar
Alcohol, without being additionally passed through hydrogen or the other reducing agents of addition.Reaction equation is as follows：
Si+2KOH+H2O=K2SiO3+2H2↑
Si+2NaOH+H2O=Na2SiO3+2H2↑
C6H12O6+H2=C6H14O6(glucose, fructose)
C5H10O5+H2=C5H12O5(xylose)
The sugar alcohol silicon solution of generation is reacted, through acid for adjusting pH, generates white carbon precipitation, reaction equation is as follows：
K2SiO3+H2SO4=H2O+SiO2↓+K2SO4
Na2SiO3+H2SO4=H2O+SiO2↓+Na2SO4
K2SiO3+ 2HCl=H2O+SiO2↓+2KCl
Na2SiO3+ 2HCl=H2O+SiO2↓+2NaCl
The glucose, xylose, the fructose starting materials that are used in the above-mentioned preparation method of the present invention are cheap to be easy to get.
It is discharged in preparation method of the present invention without waste liquid, exhaust gas, preparation process meets the theory of circular economy system.
The technical characterstic and excellent results of the present invention：
1. the preparation method of sugar alcohol of the present invention and white carbon is novel, raw material is cheap to be easy to get, and operating procedure is easy, can be applied to
Industrialization large-scale production；
2. the present invention is reducing agent using the hydrogen that silicon is generated with highly basic reaction, other without being additionally passed through hydrogen or addition
Reducing agent；
3. unreacted substance and product can reuse in preparation process in the present invention, and pollute without " three wastes ", have
Huge economic benefit and environmental benefit.
4. for sugar alcohol purity prepared by the present invention up to more than 90%, gained white carbon reaches HG/T 3061-2009 A classes
Standard.
In conclusion the method for the present invention have many advantages, such as low raw-material cost, it is simple for process, environmentally friendly, recycle, and make
The sugar alcohol purity obtained is high, white carbon large specific surface area.
Description of the drawings
Fig. 1 is the nitrogen adsorption desorption graph of white carbon prepared by embodiment 1, wherein, abscissa is adsorbance, unit：
ml/g；Ordinate is relative pressure, unit：p/po。
Specific embodiment
Further description is made to the above of the present invention below by way of specific embodiment, but this should not be managed
It solves and is only limitted to following examples for present disclosure, protection scope of the present invention is not limited to this.
It is not specified in following embodiment preparation method to implement according to the prior art.
Embodiment 1
A kind of method for preparing sugar alcohol co-producing white carbon black, step are as follows：
(1) 400Kg potassium hydroxide and 1000Kg water are added in reaction kettle, stirring at normal temperature, until no solid particle is
Only, solution A is obtained；
(2) 800Kg glucose is added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle
Until, obtain solution B；
(3) 100Kg silicon is added in the solution B of step (2) preparation, then adds in Raney's nickel 8Kg, then reaction kettle is close
Envelope, nitrogen displacement 3 times；
(4) reaction kettle is warming up to 130 DEG C, is stirred to react 5h, be cooled to room temperature, then filtered by filter, filtered
To liquor C and filter residue D, recycled in filter residue D return to step (3) reaction kettle, liquor C is sugar alcohol silicon solution.
(5) hydrochloric acid is added in into liquor C, pH to 6~7 is adjusted, is warming up to 60 DEG C, is stirred to react 60min, by filter
Filtering, is obtained by filtration filtrate E and solid F, solid F is dried, obtains white carbon.
(6) filtrate E is obtained into sorbitol solution G, solution G is concentrated, spray drying obtains sorb through electrodialysis desalination
Sugar alcohol.
Under the conditions of this, it is 93% to prepare D-sorbite purity, and 203 ㎡ of white carbon specific surface area/g reach HG/T
3061-2009A class standards.
Embodiment 2
A kind of method for preparing sugar alcohol co-producing white carbon black, step are as follows：
(1) 200Kg potassium hydroxide and 1000Kg water are added in reaction kettle, stirring at normal temperature, until no solid particle is
Only, solution A is obtained；
(2) 300Kg xyloses are added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle is
Only, solution B is obtained；
(3) 50Kg silicon is added in the solution B of step (2) preparation, then adds in palladium carbon 5Kg, then reaction kettle is sealed,
Nitrogen displacement 4 times；
(4) reaction kettle is warming up to 170 DEG C, is stirred to react 3h, be cooled to room temperature, then filtered by filter, filtered
To liquor C and filter residue D, recycled in filter residue D return to step (3) reaction kettle, liquor C is sugar alcohol silicon solution.
(5) hydrochloric acid is added in into liquor C, pH to 6~7 is adjusted, is warming up to 70 DEG C, is stirred to react 40min, by filter
Filtering, is obtained by filtration filtrate E and solid F, solid F is dried, obtains white carbon.
(6) filtrate E is obtained into xylitol solution G, solution G is concentrated, spray drying obtains xylose through electrodialysis desalination
Alcohol.
Under the conditions of this, it is 91% to prepare xylitol purity, and 197 ㎡ of white carbon specific surface area/g reach HG/T 3061-
2009A class standards.
Embodiment 3
A kind of method for preparing sugar alcohol co-producing white carbon black, step are as follows：
(1) 500Kg sodium hydroxides and 1000Kg water are added in reaction kettle, stirring at normal temperature, until no solid particle is
Only, solution A is obtained；
(2) 1000Kg glucose is added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle
Until, obtain solution B；
(3) 125Kg silicon is added in the solution B of step (2) preparation, then adds in palladium carbon 5Kg, then reaction kettle is close
Envelope, nitrogen displacement 3 times；
(4) reaction kettle is warming up to 120 DEG C, is stirred to react 15h, be cooled to room temperature, then filtered by filter, filtered
To liquor C and filter residue D, recycled in filter residue D return to step (3) reaction kettle, liquor C is sugar alcohol silicon solution.
(5) sulfuric acid is added in into liquor C, pH to 6~7 is adjusted, is warming up to 50 DEG C, is stirred to react 80min, by filter
Filtering, is obtained by filtration filtrate E and solid F, solid F is dried, obtains white carbon.
(6) filtrate E is obtained into sorbitol solution G, solution G is concentrated, spray drying obtains sorb through electrodialysis desalination
Sugar alcohol.
Under the conditions of this, it is 94% to prepare D-sorbite purity, and 225 ㎡ of white carbon specific surface area/g reach HG/T
3061-2009A class standards.
Embodiment 4
A kind of method for preparing sugar alcohol co-producing white carbon black, step are as follows：
(1) 300Kg sodium hydroxides and 1000Kg water are added in reaction kettle, stirring at normal temperature, until no solid particle is
Only, solution A is obtained；
(2) xylose 500Kg is added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle is
Only, solution B is obtained；
(3) 75Kg silicon is added in the solution B of step (2) preparation, then adds in Raney's nickel 5Kg, then reaction kettle is close
Envelope, nitrogen displacement 4 times；
(4) reaction kettle is warming up to 160 DEG C, is stirred to react 10h, be cooled to room temperature, then filtered by filter, filtered
To liquor C and filter residue D, recycled in filter residue D return to step (3) reaction kettle, liquor C is sugar alcohol silicon solution.
(5) sulfuric acid is added in into liquor C, pH to 6~7 is adjusted, is warming up to 60 DEG C, is stirred to react 50min, by filter
Filtering, is obtained by filtration filtrate E and solid F, solid F is dried, obtains white carbon.
(6) filtrate E is obtained into xylitol solution G, solution G is concentrated, spray drying obtains xylose through electrodialysis desalination
Alcohol.
Under the conditions of this, it is 92% to prepare xylitol purity, and 212 ㎡ of white carbon specific surface area/g reach HG/T 3061-
2009A class standards.
Embodiment 5
A kind of method for preparing sugar alcohol co-producing white carbon black, step are as follows：
(1) 100Kg potassium hydroxide and 1000Kg water are added in reaction kettle, stirring at normal temperature, until no solid particle is
Only, solution A is obtained；
(2) 200Kg fructose is added in step (1) in solution A obtained, stirring at normal temperature, until no solid particle is
Only, solution B is obtained；
(3) 25Kg silicon is added in the solution B of step (2) preparation, then adds in Raney's nickel 4Kg, then reaction kettle is close
Envelope, nitrogen displacement 5 times；
(4) reaction kettle is warming up to 150 DEG C, is stirred to react 7h, be cooled to room temperature, then filtered by filter, filtered
To liquor C and filter residue D, recycled in filter residue D return to step (3) reaction kettle, liquor C is sugar alcohol silicon solution.
(5) sulfuric acid is added in into liquor C, pH to 6~7 is adjusted, is warming up to 80 DEG C, is stirred to react 40min, by filter
Filtering, is obtained by filtration filtrate E and solid F, solid F is dried, obtains white carbon.
(6) filtrate E is obtained into mannitol solution G, solution G is concentrated, spray drying obtains sweet dew through electrodialysis desalination
Alcohol.
Under the conditions of this, it is 91% to prepare mannitol purity, and 204 ㎡ of white carbon specific surface area/g reach HG/T 3061-
2009A class standards.
Comparative example 1
As described in Example 1, unlike, step (4) reaction temperature is 90 DEG C.
Since temperature is too low, react and its slow.
Comparative example 2
As described in Example 1, unlike, step (4) reaction temperature is 220 DEG C.
Since temperature is excessively high, and reaction occurs in confined conditions, and reaction is violent, and pressure rise is rapid, and operation can not be controlled
System.
Claims (10)
1. a kind of method for preparing sugar alcohol co-producing white carbon black, as follows including step：
Raw material sugar with water-soluble strong base solution is mixed, adds in silicon, catalyst, deoxygenation is enclosed within 100~200 DEG C and is stirred to react；
Filtering, obtains liquor C and filter residue D；
Liquor C adds in acid, adjusts pH, is stirred to react, and filters, obtains filtrate E and solid F, solid F is dried, obtains white carbon；
By filtrate E through electrodialysis desalination, sugar alcohol solution G is obtained, sugar alcohol solution G is concentrated, spray drying obtains sugar alcohol.
2. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that it is described water solubility highly basic be
Sodium hydroxide or potassium hydroxide.
3. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that water-soluble strong base solution
In, the mass ratio of water-soluble highly basic and water is 0.1~0.5：1.
4. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that the raw material sugar is Portugal
Grape sugar, xylose or/and fructose.
5. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that raw material sugar with it is water-soluble
Property strong base solution in water mass ratio be 0.1~1：1.
6. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that the silicon and water solubility are strong
The molar ratio of alkali is 0.45~0.55：1.
7. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that the catalyst is thunder Buddhist nun
Nickel or palladium carbon；
Preferably, Ni >=90wt% in Raney's nickel, Pd >=5wt% in palladium carbon.
8. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that the catalyst and raw material
The mass ratio of sugar is 0.001~0.02：1.
9. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that silicon is added in, in catalyst
Temperature is stirred to react as 110~170 DEG C under catalysis.
10. the method according to claim 1 for preparing sugar alcohol co-producing white carbon black, which is characterized in that the acid is sulfuric acid
Or hydrochloric acid；
Preferably, it is 6~7 to adjust pH；
Preferably, it is 40~90 DEG C to adjust the temperature being stirred to react after pH.
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| CN104496653A (en) * | 2014-12-02 | 2015-04-08 | 青岛明月海藻集团有限公司 | Multi-functional sugar alcohol calcium leaf fertilizer and preparation method thereof |
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